锡试金富集-电感耦合等离子体质谱法测定黑色页岩中的铂族元素
ICP-MS Determination of Platinum Metals in Black Shale Enriched by Tin Fire Assay
摘 要
黑色页岩中的铂族元素经锡试金富集后,所得贵金属沉淀物用盐酸-硝酸(3+1)混合酸溶解,用电感耦合等离子体质谱法测定样品中的铂族元素。以镥为内标元素,用轻质氧化镁-高纯碳化硅(2+1)作覆盖剂,以防止锇和钌的挥发损失。铂族元素在一定的质量浓度范围内与其光谱强度呈线性关系,检出限(3σ)在0.018~0.20 ng·g-1之间。方法的加标回收率在80.0%~110%之间,相对标准偏差(n=11)在5.9%~14%之间。
铂族元素
锡试金
黑色页岩
ICP-MS
Platinum metals
Tin fire assay
Black shale
Abstract
Platinum metals in black shale were enriched by the method of tin fire assay. The precious metal precipitate obtained was dissolved in mixed acid of HCl-HNO3 (3+1), and contents of platinum metals in the solution were determined by ICP-MS. Lutetium was used as internal standard; and a mixture of light MgO and high purity SiC (2+1) was used as covering reagent to avoid the volatilization of Os and Ru. Linear relationships between values of spectral intensity and mass concentration of the platinum metals were kept in definite ranges. Detection limits (3σ) found were in the range of 0.018-0.20 ng·g-1. Tests for recovery were made by standard addition method, giving values of recovery in the range of 80.0%-110% with RSD′s (n=11) in the range of 5.9%-14%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 国土资源部公益性行业专项(200911043-01)
收稿日期 2013/1/20
修改稿日期
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联系人作者王君玉(junyu65@126.com)
备注王君玉(1965-),女,河南林州人,教授级高级工程师,主要从事化学分析。
引用该论文: WANG Jun-yu,SUN Zi-jun,YUAN Run-lei,WANG Ying,LI Jie,WANG Min-jie. ICP-MS Determination of Platinum Metals in Black Shale Enriched by Tin Fire Assay[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(8): 972～975
王君玉,孙自军,袁润蕾,王盈,李杰,王敏捷. 锡试金富集-电感耦合等离子体质谱法测定黑色页岩中的铂族元素[J]. 理化检验－化学分册, 2013, 49(8): 972～975
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参考文献
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【3】袁卓斌,吕元奇,张裕平,等.电感耦合等离子体质谱在铂族元素分析中的应用［J］.冶金分析, 2003,23(2):24-30.
【4】陈景.火法冶金中贱金属及锍捕集贵金属原理的讨论［J］.中国工程科学, 2007,9(5):11-15.
【5】石贵勇,孙晓明,屈文俊,等.锍镍试金富集-等离子体质谱法测定西太平洋富钴结壳中的铂族元素［J］.岩矿测试, 2007,26(2):113-116.
【6】石贵勇,孙晓明,张燕,等.锍镍试金富集-等离子体质谱法测定煌斑岩中铂族元素［J］.岩矿测试, 2008,27(4):241-244.
【7】GROS M, LORAND J P, LUGUET A. Analysis of platinum group elements and gold in geological materials using NiS fire assay and Te coprecipitation: the NiS dissolution step revisited［J］. Chemical Geology, 2002,185(3/4):179-190.
【8】EBIHARA M, LI Xiao-lin. Determination of all platinum-group elements in mantle-derived xenoliths by neutron activation analysis with Nis fire-assay preconcentration［J］. Journal of Radioanalytical and Nuclear Chemistry, 2003,255(1):131-135.
【9】BALARAM V, MATHUR R, BANAKAR V K, et al. Determination of the platinum-group elements and gold in manganese nodule reference samples bynickel sulfide fire-assay and Te coprecipitation with ICP-MS［J］. Indian Journal of Marine Sciences, 2006,35(1):7-16.
【10】VANHAECKE F, RESANO M, KOCH J, et al. Femtosecond laser ablation-ICP-mass spectrometry analysis of a heavy metallic matrix: Determination of platinum group metals and gold in lead fire-assay buttons as a case study［J］. Journal of Analytical Atomic Spectrometry, 2010,25:1259-1267.
【11】JUVONEN R, LAKOMAA T, SOIKKELI L. Determination of gold and the platinum group elements in geological samples by ICP-MS after nickel sulphide fire assay: difficulties encountered with different types of geological samples［J］. Finland Talanta, 2002,58:595-603.
【12】赵素利,张欣,温宏利,等.锍镍试金富集-电感耦合等离子体质谱法测定黑色页岩中的铂族元素［J］.岩矿测试, 2011,30(4):723-726.
【13】王君玉,毋喆,胡家祯,等.黑色岩系样品中铂族元素的分析方法［J］.黄金, 2011,31(8):723-726.
【14】王君玉,吴葆存,李志伟,等.敞口酸溶-电感耦合等离子体质谱法同时测定地质样品中45个元素［J］.岩矿测试, 2011,30(4):440-445.
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